CN100592945C - Method of making a submicron cemented carbide powder mixture with low compacting pressure - Google Patents

Method of making a submicron cemented carbide powder mixture with low compacting pressure Download PDF

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Publication number
CN100592945C
CN100592945C CN200610107585A CN200610107585A CN100592945C CN 100592945 C CN100592945 C CN 100592945C CN 200610107585 A CN200610107585 A CN 200610107585A CN 200610107585 A CN200610107585 A CN 200610107585A CN 100592945 C CN100592945 C CN 100592945C
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powder
saturated
unrighted acid
hmw
weight
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Expired - Fee Related
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CN200610107585A
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CN1903486A (en
Inventor
奥韦·阿尔姆
苏珊娜·诺格伦
阿利斯泰尔·格雷亚尔森
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Sandvik Intellectual Property AB
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • C22C29/08Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/105Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing inorganic lubricating or binding agents, e.g. metal salts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632Organic additives
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/041Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/042Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps

Abstract

The present invention relates to a method of making a ready to press cemented carbide powder with low compaction pressure suitable for the production of submicron cemented carbide by means of powder metallurgical techniques milling, pressing and sintering. The method comprises using 1 - 3 wt-% pressing agent of the following composition, <90 wt-% PEG and 10 - 75 wt-% of blends of high molecular weight (C12 - <C20) saturated or unsaturated fatty acids, or salts thereof containing at least one element of Al, Ba, Ca, Co, Cr, Mg, N, Na, V, Zn. Preferably the grain size of the cemented carbide powder is submicron. In a preferred embodiment the method includes a dry pre-milling of the hard constituents mainly WC-powder for about 2-45 hours in ball mills with cemented carbide milling bodies or using other suitable dry milling techniques prior to a wet milling step. The invention also relates to the powder obtained by the method.

Description

Low compacting pressure submicrometer hard alloy powder and manufacture method thereof
Technical field
The present invention relates to make the method and the resulting powder of the cemented carbide powder of fine fraction, especially sub-micron with low compacting pressure and nano-scale.
Background technology
Carbide alloy is by the powder that will form the hard component, forms the powder of bonding phase and be generally pressing mold agent (pressing agent) the wet-milling form slurry of PEG (polyethylene glycol), and generally coming dry slurry by spray-drying, the powder of instrument compaction drying is to the base substrate that requires shape and carry out sintering at last and make.In sintering process, the about 16-20% of base substrate linear contraction.Amount of contraction depends on pressing pressure, wc grain size, size distribution and Co content.Operated pressing tool involves great expense, and therefore with the linear contraction amount of standard, for example 18% makes.Obtain suitable amount of contraction by applying specific pressing pressure to a certain amount of powder.Sintered body have with desired approaching as far as possible size and shape be very important, to avoid expensive back sintering operation, for example grind.But, if granularity is thinner, for example be sub-micron or thinner, then need higher pressing pressure to obtain to provide the green density of necessary amount of contraction.Reach the danger that the operator is injured owing to occur the inordinate wear even the tool failure of pressure check and operated pressing tool in the base substrate after compacting, high pressing pressure is not desirable.And, if pressing pressure is remained in the particular range, will become easy to the size Control of whole sintered part(s).
EP-A-1043413 discloses the method that a kind of reduction is used for the briquetting pressure of submicrometer hard alloy.Described method comprised all components that is pre-mixed except that WC about three hours, added WC powder, and ground at last about ten hours.
Pressing mold agent commonly used in iron powder metallurgy is a zinc stearate.
Summary of the invention
An object of the present invention is to provide the method that when making fine grain carbide alloy, reduces pressing pressure.
Find surprisingly, if the mixture that uses the fatty acid cpds of blend of the salt that comprises most of higher molecular weight as unrighted acid and PEG is as the pressing mold agent, and, can obtain submicrometer hard alloy powder 18% linear contraction, that under predetermined weighing, have the briquetting pressure of reduction in conjunction with preferably under drying regime, grinding the hard component in advance.
Method of the present invention can be used to comprise the various carbide alloy of the cobalt of the cobalt of WC and/or other carbide and 2-20 weight %, preferred 5-15 weight %.It is to having the particle mean size of 0.2-1.2 μ m, preferred 0.3-1.0 μ m, be substantially free of>WC particle of 1.5 μ m and contain grain growth inhibitor, especially<1 weight % Cr and/or<submicrometer hard alloy of the V of 1 weight % is especially effective.
The specific embodiment
Thus, the present invention relates to make the method for (the ready to press) cemented carbide powder that is easy to suppress, this powder is suitable for by PM technique, i.e. wet-milling, compacting and sintering are produced submicrometer hard alloy.Wet-milling is for example to contain WC powder, other possible hard component respectively, and carry out in the ethanol of metal adhesive and pressing mold agent.Described method comprises the pressing mold agent of using 1-3 weight %, and this pressing mold agent comprises: the PEG of<90 weight %; (the saturated or unrighted acid of C12-<C20) or its contain Al, Ba, Ca, Co, Cr, Mg, N, Na, V, Zn with the HMW of 10-75 weight %, preferred 25-50 weight %, the blend of the salt of at least a element among preferred Co, Cr, N, V or the Zn, preferably come drying, be pressed into the base substrate that requires shape and sinter densification, homogeneous, high performance carbide chip into by spray-drying.
In a preferred embodiment of the invention, process of lapping is from the pre-grinding step, wherein uses ball milling with carbide alloy abrasive body or other dry mill process that is fit to dry grind and forms powder 2-45 hour of the hard component.The dry grinding time that needs is depended on the final pressing pressure or the amount of contraction of size, powder size and the requirement of mill, and those skilled in the art can easily determine.The pre-grinding step is succeeded by aforesaid final wet-milling step.
The invention still further relates to and be used for the powder making carbide alloy, be easy to suppress with low compacting pressure.This powder contains the pressing mold agent of the following composition of 1-3 weight %: the PEG of weight % promptly<90; With the HMW of 10-75 weight %, preferred 25-50 weight % (the saturated or unrighted acid of C12-<C20), or it contains Al, Ba, Ca, Co, Cr, Mg, N, Na, V, Zn, the blend of the salt of at least a element among preferred Co, Cr, N, V or the Zn.In a preferred embodiment, the granularity of powder is a submicron order.
Embodiment 1
The submicron cemented carbide powder mixture of the composition of the Co of Cr, the 6 weight % of WC, the 0.3 weight % with 0.8 μ m average grain diameter produced according to the present invention.Grinding is to carry out in ethanol (every kilogram of cemented carbide powder 0.3 up-flow body) in having 2.5 liters of laboratory grinders of 8 kilograms of abrasive bodies, and the batch of material amount is 2 kilograms.Use following pressing mold agent:
1A:PEG 40g (prior art)
1B:PEG 28g and major part are the blend 12g of zinc salt of the higher molecular weight of unrighted acid
After the spray-drying, according to the blade of standard operation compacting and sintering SNUN120408.In the pressing operation process, get the mean value of six blades, the record briquetting pressure is following result:
The sample briquetting pressure, MPa
1A 155
1B 77
Embodiment 2
The WC powder that use was dry grinded 12 hours in having small-sized 2.5 liters of laboratory grinders of 8 kilograms of abrasive bodies and 2.0 kilograms of WC powders in advance repeats embodiment 1.Obtain following pressing pressure:
The sample briquetting pressure, MPa
2A 130
2B 47
Sintering blade among these two embodiment is carried out the metallurgical check of routine.Obtain fine and close sintered configuration, do not found the sign of hole or pressure check.But, to much lower than among the embodiment 1 of the pressing pressure of the sample among the embodiment 2 record.And the pressing pressure of finding to be used for sample 1B and 2B is than pairing sample, promptly only contains PEG much lower as the 1A of pressing mold agent and 2A.These find to be undoubtedly favourable to the life-span of operated pressing tool.
Embodiment 3
The submicron cemented carbide powder mixture of the composition of the Co of Cr, the 10 weight % of WC, the 0.5 weight % with 0.3 μ m average grain diameter produced according to the present invention.Grinding is to carry out in ethanol (every kilogram of cemented carbide powder 0.3 up-flow body) in having 2.5 liters of laboratory grinders of 8 kilograms of abrasive bodies, and the batch of material amount is 2 kilograms.Use following pressing mold agent:
3A:PEG 40g (prior art)
3B:PEG 25g and major part are the blend 15g of zinc salt of the higher molecular weight of unrighted acid
3C:PEG 25g and cobaltous octadecanate 15g
3D:PEG 28g and oleic acid 12g
After the spray-drying, according to the blade of standard operation compacting and sintering SNUN120408.In the pressing operation process, under 0.55 relative green density, get the mean value of six blades, the record briquetting pressure is following result:
The sample briquetting pressure, MPa
3A 550
3B 450
3C 490
3D 460
The sintering blade is carried out the metallurgical check of routine.Except that sample 3A, obtained fine and close sintered configuration, and do not found pressure check or more macroporous sign.
Embodiment 4
The WC powder that use was dry grinded 35 hours in having small-sized 2.5 liters of laboratory grinders of 8 kilograms of abrasive bodies and 2.0 kilograms of WC powders in advance repeats embodiment 3.When the relative green density that is pressed into 0.55, obtain following pressing pressure:
The sample briquetting pressure, MPa
4A 195
4B 120
4C 140
4D 130
The sintering blade is carried out the metallurgical check of routine.In 4A-4D, obtain fine and close sintered configuration, do not had to find the bigger hole or the sign of pressure check.But, to much smaller than among the embodiment 3 of the pressing pressure of the sample among the embodiment 4 record.The pressing pressure that we also find to be used for sample 4B-4D is starkly lower than and is used for only containing the pressure of PEG as the sample 4A of pressing mold agent.These find that the danger for wearing and tearing that minimize operated pressing tool and tool failure undoubtedly is important.

Claims (10)

1. make the method for the cemented carbide powder that is easy to suppress, described cemented carbide powder is suitable for passing through PM technique, promptly grind, compacting and sintering, comprise wet-milling, make submicrometer hard alloy, it is characterized in that, use the pressing mold agent of the following composition of 1-3 weight %: the polyethylene glycol of weight % promptly<90; The blend of or unrighted acid saturated with the HMW of 10-75 weight %, or described HMW is saturated or the blend of the salt that contains at least a element among Al, Ba, Ca, Co, Cr, Mg, N, Na, V, the Zn of unrighted acid, the carbon number of the saturated or unrighted acid of wherein said HMW is more than or equal to 12, and less than 20.
2. according to the method for claim 1, the granularity that it is characterized in that described cemented carbide powder is a submicron order.
3. according to the method for claim 1, it is characterized in that, before the wet-milling step, in ball milling, dry grind in advance and be mainly the about 2-45 of hard component hour of WC powder with carbide alloy abrasive body.
4. according to the method for claim 1, it is characterized in that in the ethanol that contains WC powder and other possible hard component powders, metal adhesive and pressing mold agent, carrying out wet-milling.
5. according to the method for claim 1, it is characterized in that the blend of the saturated or unrighted acid of described HMW, or described HMW is saturated or the blend of the described salt of unrighted acid is 25-50 weight %.
6. according to the method for claim 1, it is characterized in that described salt saturated or unrighted acid contains at least a element among Co, Cr, N, V or the Zn.
7. be used for the powder making carbide alloy, be easy to suppress with low compacting pressure, it is characterized in that, contain the pressing mold agent of the following composition of 1-3 weight %: the polyethylene glycol of weight % promptly<90; The blend of or unrighted acid saturated with the HMW of 10-75 weight %, or described HMW is saturated or the blend of the salt that contains at least a element among Al, Ba, Ca, Co, Cr, Mg, N, Na, V, the Zn of unrighted acid, the carbon number of the saturated or unrighted acid of wherein said HMW is more than or equal to 12, and less than 20.
8. according to the powder of claim 7, the granularity that it is characterized in that cemented carbide powder is a submicron order.
9. according to the powder of claim 7, it is characterized in that the blend of the saturated or unrighted acid of described HMW, or described HMW is saturated or the blend of the described salt of unrighted acid is 25-50 weight %.
10. according to the powder of claim 7, it is characterized in that described HMW salt saturated or unrighted acid contains at least a element among Co, Cr, N, V or the Zn.
CN200610107585A 2005-07-29 2006-07-27 Method of making a submicron cemented carbide powder mixture with low compacting pressure Expired - Fee Related CN100592945C (en)

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SE05017462 2005-07-29
SE0501746A SE529297C2 (en) 2005-07-29 2005-07-29 Ways to make a submicron cemented carbide powder mixture with low compression pressure

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US (1) US8425652B2 (en)
EP (1) EP1749601B1 (en)
JP (1) JP5324033B2 (en)
KR (1) KR101278350B1 (en)
CN (1) CN100592945C (en)
AT (1) ATE392967T1 (en)
DE (1) DE602006000982T2 (en)
IL (1) IL176536A (en)
SE (1) SE529297C2 (en)

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SE533912C2 (en) * 2009-02-19 2011-03-01 Seco Tools Ab Fine-grained cemented carbide powder mixture with low sintering shrinkage and method of manufacturing the same
EP2246113A1 (en) * 2009-04-29 2010-11-03 Sandvik Intellectual Property AB Process for milling cermet or cemented carbide powder mixtures
JP5519430B2 (en) * 2010-06-30 2014-06-11 株式会社日立製作所 Manufacturing method of MgB2 superconducting wire
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CN102389857A (en) * 2011-09-19 2012-03-28 常州大学 Mixed preparation method of nanometer powder and non-nanometer powder
JP5889116B2 (en) * 2012-06-11 2016-03-22 株式会社日立製作所 MgB2 superconducting wire and method for producing the same
CN103008666A (en) * 2012-12-27 2013-04-03 遵义中铂硬质合金有限责任公司 Production technique for hard alloy cold heading die
CN105154746A (en) * 2015-09-07 2015-12-16 南京腾达五金制品有限公司 High temperature resistant alloy cutter head and preparation method thereof
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EP1749601A1 (en) 2007-02-07
KR101278350B1 (en) 2013-06-25
DE602006000982D1 (en) 2008-06-05
EP1749601B1 (en) 2008-04-23
KR20070015030A (en) 2007-02-01
ATE392967T1 (en) 2008-05-15
DE602006000982T2 (en) 2009-06-10
JP5324033B2 (en) 2013-10-23
CN1903486A (en) 2007-01-31
SE529297C2 (en) 2007-06-26
JP2007039810A (en) 2007-02-15
US20070025872A1 (en) 2007-02-01
IL176536A0 (en) 2006-10-05
SE0501746L (en) 2007-01-30
US8425652B2 (en) 2013-04-23

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